CN115161568B - Anti-pulverization block getter and preparation method thereof - Google Patents
Anti-pulverization block getter and preparation method thereof Download PDFInfo
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- CN115161568B CN115161568B CN202210837105.7A CN202210837105A CN115161568B CN 115161568 B CN115161568 B CN 115161568B CN 202210837105 A CN202210837105 A CN 202210837105A CN 115161568 B CN115161568 B CN 115161568B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
- C22C47/14—Making alloys containing metallic or non-metallic fibres or filaments by powder metallurgy, i.e. by processing mixtures of metal powder and fibres or filaments
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
- C22C49/02—Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
- C22C49/10—Refractory metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
- C22C49/14—Alloys containing metallic or non-metallic fibres or filaments characterised by the fibres or filaments
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
Abstract
The application provides a preparation method of an anti-pulverization block getter, which comprises the following steps: preparing raw materials in the getter alloy according to a certain proportion, preparing the alloy by a smelting method, and then crushing and ball-milling the alloy in a protective atmosphere; uniformly mixing getter alloy powder with titanium and titanium alloy fibers in a certain proportion to form an alloy mixture; pressing the alloy mixture in a rigid die to form a pressed compact; in a vacuum degree of 3 to 5 multiplied by 10 ‑3 And (3) carrying out vacuum sintering on the pressed compact in a vacuum environment of Pa to obtain the block getter with strong pulverization resistance. The bulk getter product produced by the application has better toughness in MEMS wafer level packaging, overcomes the phenomenon of powder and slag falling in the use process of the product, can maintain better vacuum degree in a vibration environment after wafer packaging, is beneficial to prolonging the service life, has simple structural design, is suitable for mass production, and can effectively meet the demands of users.
Description
The application relates to a divisional application of a preparation method of an anti-pulverization block getter, wherein the application date is 2019, 10, 16, the application number is 201910983452.9.
Technical Field
The application relates to the field of MEMS wafer level high-vacuum packaging, in particular to an anti-pulverization block getter and a preparation method thereof.
Background
The coming of the 'Internet of things' age has increased the demand for intelligent chips, and the development of MEMS (Micro-Electro-Mechanical System) devices has been raised worldwide. As a key material used for MEMS device vacuum packaging, the parameters of the air suction performance, the bonding strength with a wafer matrix and the like become key technical indexes for influencing the sensitivity and the stability of the MEMS device.
The getter is needed for the MEMS device because the getter can improve the vacuum degree of the device after being placed in the MEMS device for vacuum packaging, thereby greatly improving the sensitivity, safety, stability and reliability of the MEMS device. The MEMS device comprises a mechanical moving part, if the vacuum environment is not good, the part can be damped by gas in the moving process, so that the device consumes redundant energy, and more importantly, the Q value of the device can be reduced along with the increase of pressure, thereby influencing the performance of the MEMS device. If the free particles have a relatively long molecular mean free path in a high vacuum environment, the conduction heat transfer can be inhibited; meanwhile, the high vacuum can improve the breakdown voltage of an air gap, and the high efficiency and long service life of the MEMS device are ensured.
The main function of the getter material is to absorb the residual gas remained in the vacuum electronic device, especially the deionization vacuum tube during or after mechanical exhaustion, to improve the vacuum degree in the tube, ensure the normal operation of the device, prolong the service life and improve the reliability of the device. The high vacuum environment requires a bulk getter material with high gettering efficiency, so it is important to invent a getter material with high gettering efficiency and resistance to pulverization under moving conditions or vibration environment.
Disclosure of Invention
The application aims to provide an anti-pulverization block getter with high gettering efficiency and long service life and a preparation method thereof.
The purpose of the application is realized in the following way: a preparation method of an anti-pulverization block getter comprises the following steps:
1) Preparing raw materials in the getter alloy according to a certain proportion, preparing the alloy by a smelting method, and then crushing and ball-milling the alloy under a protective atmosphere to obtain getter alloy powder with 300-80 meshes;
2) Uniformly mixing the getter alloy powder with 0.1-70 wt% of titanium and titanium alloy fibers to form an alloy mixture;
3) Pressing the alloy mixture in a rigid die to form a pressed compact;
4) In a vacuum degree of 3 to 5 multiplied by 10 -3 Vacuum sintering the pressed compact in a vacuum environment of Pa to obtain the anti-pulverization productA bulk getter;
the getter alloy is Zr56.97V35.85Cr7.18 or Zr30Ti3.33V66.69; the diameter of the titanium and titanium alloy fiber is 0.04-0.09 mm, and the length is 0.2-2 mm.
Preferably, the pressing pressure is 1-200 Mpa, the pressing dwell time is 1-30 s, and the relative density of the pressed compact is 30-60%.
Preferably, the temperature of the vacuum sintering is 900-1030 ℃, and the heat preservation time of the vacuum sintering is 0.2-2 h.
The application also provides the anti-pulverization block getter prepared by the preparation method.
Drawings
Fig. 1 is a diagram of titanium and titanium alloy fibers.
Detailed Description
The following description of the embodiments of the present application will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
The preparation method of the anti-pulverization block getter comprises the following steps:
1) Preparing raw materials in the getter alloy according to a certain proportion, preparing the alloy by a smelting method, and then crushing and ball-milling the alloy under a protective atmosphere to obtain getter alloy powder with 300-80 meshes;
2) Uniformly mixing the getter alloy powder with 0.1-70 wt% of titanium and titanium alloy fibers to form an alloy mixture;
3) Pressing the alloy mixture in a rigid die to form a pressed compact;
4) In a vacuum degree of 3 to 5 multiplied by 10 -3 And (3) carrying out vacuum sintering on the pressed compact in a vacuum environment of Pa to obtain the block getter with strong pulverization resistance.
The types of the above alloys include:
a) Zr-Al alloy, zr-Al-RE alloy, zr-Al-TE-RE alloy, wherein TE comprises transition group element Ti, fe, co, ni, mn, pd, ru, pt, V, cr, nb, mo, tc, rh, hf, ta, W, re, os, ir;
b) Zr-C alloy, zr-C-RE alloy, zr-C-TE-RE alloy, wherein TE comprises transition group element Ti, fe, co, ni, mn, pd, ru, pt, V, cr, nb, mo, tc, rh, hf, ta, W, re, os, ir;
c) Zr-V-Fe alloy, zr-V-Fe-RE alloy, zr-V-Fe-TE alloy, zr-V-Fe-RE-TE alloy, wherein TE comprises transition group element Ti, co, ni, mn, pd, ru, pt, cr, nb, mo, tc, rh, hf, ta, W, re, os, ir;
d) Zr-Co alloy, zr-Co-RE alloy, zr-Co-TE alloy, zr-Co-RE-TE alloy, wherein TE comprises transition group element Ti, fe, ni, mn, pd, ru, pt, V, cr, nb, mo, tc, rh, hf, ta, W, re, os, ir;
e) Ti-Mo alloy, ti-Mo-RE alloy, ti-Mo-TE alloy, ti-Mo-RE-TE alloy, wherein TE comprises transition group element Zr, fe, co, ni, mn, pd, ru, pt, V, cr, nb, tc, rh, hf, ta, W, re, os, ir;
f) Ti-Zr-V alloy, ti-Zr-V-RE alloy, ti-Zr-V-TE-RE alloy, wherein TE comprises transition group element Fe, co, ni, mn, pd, ru, pt, cr, nb, mo, tc, rh, hf, ta, W, re, os, ir. The method comprises the steps of carrying out a first treatment on the surface of the
g) Zr-Co-Re (rhenium) alloys, zr-Co-Re- -RE- -TE alloys, where TE comprises transition group elements Ti, fe, co, ni, mn, pd, ru, pt, V, cr, nb, mo, tc, rh, hf, ta, W, os, ir.
The RE is a rare earth element Y, sc, la, ce, pr, nd, pm, sm, eu, gd, tb, dy, ho, er, tm, yb, lu.
The diameter of the titanium and titanium alloy fiber is 0.04-0.09 mm, and the length is 0.2-2 mm.
The weight ratio of the titanium and titanium alloy fiber is 0.1-70 wt%.
The molding pressure of the titanium and titanium alloy fiber and the getter alloy powder is 1-200 Mpa, the pressure is maintained for 1-30 s, and the relative density of the pressed compact is 30-60%.
The sintering process of the pressed compact is to keep the temperature for 0.2 to 2 hours at 900 to 1030 ℃.
Example 1
Based on a stoichiometric formula of Zr56.97V35.85Cr7.18 (weight ratio), preparing an alloy cast ingot through a vacuum induction smelting method, homogenizing the alloy cast ingot at 1100 ℃ for 5 hours for heat treatment, then rapidly cooling to room temperature, crushing and ball-milling the cooled cast ingot to 325-200 mesh powder, shearing titanium alloy fibers in fig. 1, and mixing the crushed titanium alloy fibers with air suction powder according to the following steps of 1:9, mixing, loading the powder into a rigid mold, pressing under 50Mpa to obtain pressed compact, loading the pressed compact into a vacuum sintering furnace, and sintering to 3.5X10 -3 Pa, sintering process is 1000 ℃ multiplied by 1h. Generating a high-strength porous getter material: after activation for 15min at 480 ℃, the total hydrogen absorption is: 201cm 3 ·Pa/g。。
Example 2
Based on a stoichiometric formula of Zr30Ti3.33V66.69 (weight ratio), preparing an alloy cast ingot through vacuum induction smelting, homogenizing and heat treating the alloy cast ingot at 1050 ℃ for 6 hours, then rapidly cooling to room temperature, crushing and ball-milling the cooled cast ingot to 325-200 mesh powder, shearing titanium alloy fibers in fig. 1, and mixing the crushed titanium alloy fibers with air suction powder according to the following ratio of 8:92, mixing, loading the powder into rigid mold, pressing under 100Mpa to obtain pressed compact, loading the pressed compact into vacuum sintering furnace, and sintering at vacuum degree of 3×10 -3 Pa, and 1020 ℃ multiplied by 1h of sintering process. Generating a high-strength porous getter material, wherein after the material is activated for 20min at 380 ℃, the total hydrogen absorption amount is as follows: 137cm 3 ·Pa/g。
The application is not limited to the above embodiments, and based on the technical solution disclosed in the application, a person skilled in the art may make some substitutions and modifications to some technical features thereof without creative effort according to the technical content disclosed, and all the substitutions and modifications are within the protection scope of the application.
Claims (4)
1. The preparation method of the anti-pulverization block getter is characterized by comprising the following steps:
1) Preparing raw materials in the getter alloy according to a certain proportion, preparing the alloy by a smelting method, and then crushing and ball-milling the alloy under a protective atmosphere to obtain getter alloy powder with 300-80 meshes;
2) Uniformly mixing the getter alloy powder with 0.1-70 wt% of titanium and titanium alloy fibers to form an alloy mixture;
3) Pressing the alloy mixture in a rigid die to form a pressed compact; the pressing pressure is 1-200 MPa;
4) In a vacuum degree of 3 to 5 multiplied by 10 -3 Vacuum sintering the pressed compact in a vacuum environment of Pa to obtain the anti-pulverization block getter;
the getter alloy is Zr 56.97 V 35.85 Cr 7.18 The method comprises the steps of carrying out a first treatment on the surface of the The diameter of the titanium and titanium alloy fiber is 0.04-0.09 mm, and the length is 0.2-2 mm.
2. The method of claim 1, wherein the pressing dwell time is 1 to 30 seconds and the relative density of the compact is 30 to 60%.
3. The method according to claim 1, wherein the temperature of the vacuum sintering is 900-1030 ℃, and the heat preservation time of the vacuum sintering is 0.2-2 h.
4. An anti-pulverization block getter prepared by the preparation method of any one of claims 1 to 3.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210837105.7A CN115161568B (en) | 2019-10-16 | 2019-10-16 | Anti-pulverization block getter and preparation method thereof |
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| CN201910983452.9A CN110616388A (en) | 2019-10-16 | 2019-10-16 | Preparation method of anti-pulverization block getter |
| CN202210837105.7A CN115161568B (en) | 2019-10-16 | 2019-10-16 | Anti-pulverization block getter and preparation method thereof |
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| CN113428830A (en) * | 2021-05-26 | 2021-09-24 | 上海晶维材料科技有限公司 | Low-activation-temperature high-performance air suction film |
| CN115449690B (en) * | 2022-09-20 | 2023-06-06 | 浙江安胜科技股份有限公司 | Zr-V series getter material with high strength and high gettering performance and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3728108A (en) * | 1969-03-31 | 1973-04-17 | Combustible Nucleaire | Process for the production of reinforced composite alloys |
| CN85109681A (en) * | 1984-12-28 | 1986-06-10 | 宇部兴产株式会社 | The manufacturing equipment of compound material |
| WO1991017277A1 (en) * | 1990-05-10 | 1991-11-14 | Lanxide Technology Company, Lp | Internal shaping techniques for metal matrix composites |
| US5439627A (en) * | 1990-06-29 | 1995-08-08 | Flexline Services Ltd. | Process for manufacturing reinforced composites |
| CN106435409A (en) * | 2016-09-26 | 2017-02-22 | 太原理工大学 | Preparation method of neutron absorbing composite material |
| CN108149069A (en) * | 2016-12-02 | 2018-06-12 | 北京有色金属研究总院 | A kind of getter alloy material and its application |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5734226A (en) * | 1992-08-12 | 1998-03-31 | Micron Technology, Inc. | Wire-bonded getters useful in evacuated displays |
| JP3698148B2 (en) * | 2003-04-28 | 2005-09-21 | 日産自動車株式会社 | Evaporable getter and vacuum vessel |
| CN103588595B (en) * | 2013-11-15 | 2015-09-09 | 中国工程物理研究院化工材料研究所 | Steel fiber toughen and intensify TNT base castexplosive and preparation method thereof |
| CN105477681A (en) * | 2015-12-31 | 2016-04-13 | 常州市长宇实用气体有限公司 | Preparation method of titanium polymer fiber-reinforced porous magnesium-based medical material |
-
2019
- 2019-10-16 CN CN201910983452.9A patent/CN110616388A/en active Pending
- 2019-10-16 CN CN202210837105.7A patent/CN115161568B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3728108A (en) * | 1969-03-31 | 1973-04-17 | Combustible Nucleaire | Process for the production of reinforced composite alloys |
| CN85109681A (en) * | 1984-12-28 | 1986-06-10 | 宇部兴产株式会社 | The manufacturing equipment of compound material |
| WO1991017277A1 (en) * | 1990-05-10 | 1991-11-14 | Lanxide Technology Company, Lp | Internal shaping techniques for metal matrix composites |
| US5439627A (en) * | 1990-06-29 | 1995-08-08 | Flexline Services Ltd. | Process for manufacturing reinforced composites |
| CN106435409A (en) * | 2016-09-26 | 2017-02-22 | 太原理工大学 | Preparation method of neutron absorbing composite material |
| CN108149069A (en) * | 2016-12-02 | 2018-06-12 | 北京有色金属研究总院 | A kind of getter alloy material and its application |
Non-Patent Citations (1)
| Title |
|---|
| 施慧生.《材料概论》.同济大学出版社,2009,第143-144页. * |
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| CN115161568A (en) | 2022-10-11 |
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